CN110273297B - 一种通过层层自组装制备pH变色纺织品的方法 - Google Patents

一种通过层层自组装制备pH变色纺织品的方法 Download PDF

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CN110273297B
CN110273297B CN201910536715.1A CN201910536715A CN110273297B CN 110273297 B CN110273297 B CN 110273297B CN 201910536715 A CN201910536715 A CN 201910536715A CN 110273297 B CN110273297 B CN 110273297B
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孙晓竹
关昶
郝凤岭
王海东
马晓坤
梁春爽
刘群
李祥
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Abstract

本发明涉及一种pH变色纺织品的制备方法，属于纺织品功能整理领域，该方法包括季铵盐壳聚糖的合成、织物的阳离子改性、pH指示剂与聚电解质在织物表面的吸附三个步骤。该方法可采用阳离子或阴离子型指示剂，通过带有不同电荷化合物间的静电引力，实现指示剂分子与织物的吸附固定，并通过引入聚电解质，在织物表面形成多层结构，提高稳定性、减少泄露。

Description

一种通过层层自组装制备pH变色纺织品的方法
技术领域
本发明属于纺织品功能整理领域，特别涉及一种通过层层自组装制备pH变色纺织品的方法。
背景技术
静电层层自组装技术主要是基于聚电解质阴阳离子所带不同电荷相互作用的一种组装分子技术，其主要方法是将表面带电基材通过静电作用交替吸附聚电解质带电离子或粒子，由于反应可在室温下进行，其聚电解质组装膜组成精确可控，具有稳定性好，操作简单，不受基材形状大小的限制等优点。目前在纺织方面，人们利用这种技术制备了电磁屏蔽、防火阻燃、去污抗菌等织物，这些尝试为其在pH变色功能化方面的实践提供了依据。
pH敏感型变色材料，是离子变色材料的一个分支，其颜色会根据 pH值的变化发生变化。pH变色织物可应用于多种场合，如用于警告腐蚀性气体存在的防护服，指示伤口愈合情况的变色绷带，测量土壤pH值的农用纺织品等。
目前，主要是通过以染色与溶胶整理的方法制备pH变色纺织品。由于pH指示剂分子结构较小，且不存在能与纤维反应的活性基团，所以染色型织物的指示剂易泄露，稳定性较差。对于整理型织物来说，由于溶胶疏水只能包裹疏水型指示剂，其变色范围与应用领域受到了限制。
发明内容
本发明所要解决的技术问题是提供一种通过层层自组装制法制备pH变色纺织品的方法，该方法通过静电引力将指示剂、聚电解质与织物结合在一起，赋予了指示剂稳定性，拓展了应用范围。
本发明的目的是这样实现的，一种层层自组装pH变色纺织品的制备方法，包括：
（1）、季铵盐壳聚糖（QCS）的制备：将1g壳聚糖溶于100 mL蒸馏水中，升至定温，加入一定量的2,3-环氧丙基三甲基氯化铵，搅拌一段时间得反应液，将反应液加入3倍体积的乙醇中，搅拌至沉淀，过滤烘干得到季铵盐壳聚糖（QCS）；
（2）、织物的阳离子改性：将一定量的3-氯-2-羟基丙基三甲基氯化铵加入200mL蒸馏水中，升至一定温度，加入4g氢氧化钠，搅拌至溶解，向整理液中投入10g织物，浸渍一段时间，取出水洗晾干，得到阳离子改性织物。
（3）、pH变色织物制备：配制一定质量浓度的QCS溶液、聚苯乙烯磺酸钠（PSS）溶液、阳离子型pH指示剂溶液与阴离子型pH指示剂溶液；
pH变色织物A的制备：室温下，先将阳离子改性织物浸渍在PSS溶液中一定时间，蒸馏水漂洗，60℃烘干，继续在阳离子型pH指示剂溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，最后在QCS溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，上述步骤视为完成一层组装，重复组装直至达到一定层数，然后将织物放入一定浓度的戊二醛溶液中，二浸二轧，60℃烘干，特定温度下焙烘一段时间得到pH变色织物A；
pH变色织物B的制备：室温下，先将阳离子改性织物浸渍在PSS溶液中一定时间，蒸馏水漂洗，60℃烘干，继续在QCS溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，最后在阴离子型pH指示剂溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，上述步骤视为完成一层组装，重复组装直至达到一定层数，然后将织物放入一定浓度的戊二醛溶液中，二浸二轧，60℃烘干，特定温度下焙烘一段时间得到pH变色织物B。
所述步骤（1）中的的反应温度为60-85℃，搅拌时间为12-48h，2,3-环氧丙基三甲基氯化铵用量为3-5g。
所述步骤（2）中的织物为棉、羊毛、蚕丝，3-氯-2-羟基丙基三甲基氯化铵用量为4-10g，温度为30-60℃，浸渍时间为40-120min。
所述步骤（3）中的QCS与PSS溶液的浓度为1-5g/L，pH指示剂浓度为0.05-0.5g/L，三次浸渍时间均为20-40分钟，组装层数为5-20层。
所述步骤（3）中阴离子型pH指示剂为灿烂黄、甲基橙、溴甲酚绿钠盐、溴百里香酚蓝钠盐，阳离子型pH指示剂为刚果红、中性红。
所述步骤（3）中，所用戊二醛溶液的浓度为0.5-5wt%，带液率为70-85%，焙烘温度为120-140℃，焙烘时间为1-3分钟。
有益效果：
(1)本发明采用两种聚电解质，可分别吸附阳离子与阴离子型pH指示剂，增加了对指示剂的选择范围，拓展了变色织物的应用领域。
(2)本发明在织物表面形成交联叠层结构，以静电引力与物理包覆对指示剂分子进行固定，减少了指示剂分子的泄露，提高了变色织物的稳定性。
附图说明
图1为本发明实施例2所得变色织物（10层）在不同pH值下的反射光谱。
图2 为本发明实施例2中不同pH值下的变色织物（10层）。
图3为本发明实施例2中变色织物（0层、5层、10层）在缓冲液中浸渍后的K/S值。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
将1g壳聚糖溶于100 mL蒸馏水中，升至70℃，加入4g的2,3-环氧丙基三甲基氯化铵，搅拌反应48h，将反应液加入300倍体积的乙醇中，搅拌至沉淀，过滤，45℃烘干。
将8g 3-氯-2-羟基丙基三甲基氯化铵加入200mL蒸馏水中，升至50温度，加入4g氢氧化钠，向整理液中投入10g棉织物，浸渍50min时间，取出水洗晾干得阳离子棉织物。
配制5g/L的QCS水溶液、5g/L的PSS水溶液与0.1g/L的中性红水溶液。将阳离子棉织物浸渍在PSS溶液中20min，水洗烘干，继续在中性红溶液中浸渍30min，水洗烘干，最后在QCS溶液中浸渍20min，水洗烘干。重复组装至5层，然后将织物放入2.5wt%的戊二醛溶液中，二浸二轧，带液率75%，烘干后130℃焙烘3min。
实施例2
将1g壳聚糖溶于100 mL蒸馏水中，升至85℃，加入4g的2,3-环氧丙基三甲基氯化铵，搅拌反应36h，将反应液加入300倍体积的乙醇中，搅拌至沉淀，过滤，45℃烘干。
将6g 3-氯-2-羟基丙基三甲基氯化铵加入200mL蒸馏水中，升至60温度，加入4g氢氧化钠，向整理液中投入10g棉织物，浸渍60min时间，取出水洗晾干得阳离子棉织物。
配制3g/L的QCS水溶液、3g/L的PSS水溶液与0.05g/L的灿烂黄水溶液。将阳离子棉织物浸渍在PSS溶液中20min，水洗烘干，继续在QCS溶液中浸渍20min，水洗烘干，最后在灿烂黄溶液中浸渍30min，水洗烘干。重复组装，分别得到0层、5层与10层变色织物，然后将织物放入1wt%的戊二醛溶液中，二浸二轧，带液率80%，烘干后140℃焙烘3min。
图1为实施例2中变色织物（10层）在不同pH下的反射光谱，由图可知，在pH值由5到8的变化过程中，织物对490-580nm区域绿色光的吸收不断增加，即提高了绿色光补色在整体颜色中所占的比例，故织物呈现出由黄至红的颜色变化，这一点同图2中的拍摄图片是一致的，图3为不同组装层数变色织物（0层、5层、10层）在pH=4与pH=9缓冲液中浸渍2h后的K/S值，由图可知，在酸性或碱性条件下，增加组装层数均可提高指示剂的稳定性，减少泄露。

Claims (1)

1.一种通过层层自组装制备pH变色纺织品的方法，该方法包括以下步骤：
(1)、季铵盐壳聚糖(QCS)的制备：将1g壳聚糖溶于100mL蒸馏水中，升至定温，加入一定量的2,3-环氧丙基三甲基氯化铵，搅拌一段时间得反应液，将反应液加入3倍体积的乙醇中，搅拌至沉淀，过滤烘干得到季铵盐壳聚糖(QCS)；
(2)、织物的阳离子改性：将一定量的3-氯-2-羟基丙基三甲基氯化铵加入200mL蒸馏水中，升至一定温度，加入4g氢氧化钠，搅拌至溶解，向整理液中投入10g织物，浸渍一段时间，取出水洗晾干，得到阳离子改性织物；
(3)、pH变色织物制备：配制一定质量浓度的QCS溶液、聚苯乙烯磺酸钠(PSS)溶液、阳离子型pH指示剂溶液与阴离子型pH指示剂溶液；
pH变色织物A的制备：室温下，先将阳离子改性织物浸渍在PSS溶液中一定时间，蒸馏水漂洗，60℃烘干，继续在阳离子型pH指示剂溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，最后在QCS溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，上述步骤视为完成一层组装，重复组装直至达到一定层数，然后将织物放入一定浓度的戊二醛溶液中，二浸二轧，60℃烘干，特定温度下焙烘一段时间得到pH变色织物A；
pH变色织物B的制备：室温下，先将阳离子改性织物浸渍在PSS溶液中一定时间，蒸馏水漂洗，60℃烘干，继续在QCS溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，最后在阴离子型pH指示剂溶液中浸渍一段时间，蒸馏水漂洗，60℃烘干，上述步骤视为完成一层组装，重复组装直至达到一定层数，然后将织物放入一定浓度的戊二醛溶液中，二浸二轧，60℃烘干，特定温度下焙烘一段时间得到pH变色织物B；
所述步骤(1)中的反应温度为60-85℃，搅拌时间为12-48h，2,3-环氧丙基三甲基氯化铵用量为3-5g；
所述步骤(2)中的织物为棉、羊毛、蚕丝，3-氯-2-羟基丙基三甲基氯化铵用量为4-10g，温度为30-60℃，浸渍时间为40-120min；
所述步骤(3)中的QCS与PSS溶液的浓度为1-5g/L，pH指示剂浓度为0.05-0.5g/L，三次浸渍时间均为20-40分钟，组装层数为5-20层；
所述步骤(3)中阴离子型pH指示剂为灿烂黄、甲基橙、溴甲酚绿钠盐、溴百里香酚蓝钠盐，阳离子型pH指示剂为刚果红、中性红；
所述步骤(3)中，所用戊二醛溶液的浓度为0.5-5wt％，带液率为70-85％，焙烘温度为120-140℃，焙烘时间为1-3分钟。
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